反应详情

5-Chloro-4-(6-chloro-3′-fluoro-4-(pyridazin-4-yl)biphenyl-3-yloxy)-N-(2,4-dimethoxybenzyl)-2-fluoro-N-(1,3,4-thiadiazol-2-yl)benzenesulfonamide (Preparation 97, 60 mg, 0.08 mmol) was dissolved in a 4M solution of HCl in dioxane (5 mL). The reaction was stirred for 18 hours at room temperature and then evaporated in vacuo. The residue was dissolved in ethyl acetate (5 mL) washed with water (2×5 mL), dried over MgSO4, filtered and concentrated in vacuo. The residue was purified by flash chromatography eluting with dichloromethane:methanol:acetic acid (97:2.7:0.3) to give 30 mg of the title compound. The compound was further purified by preparative HPLC to give the title compound (3.6 mg, 7.5%) as a solid.

1. customevaporated in vacuo
2. dissolutionThe residue was dissolved in ethyl acetate (5 mL)
3. washwashed with water (2×5 mL)
4. dry with materialdried over MgSO4
5. filtrationfiltered
6. concentrationconcentrated in vacuo
7. customThe residue was purified by flash chromatography
8. washeluting with dichloromethane:methanol:acetic acid (97:2.7:0.3)